BK4 (2b4m) Containing 4-methylpropihenon

HIGGS BOSSON

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Describe the synthesis technique you used.
Who is the supplier?
In appearance, BK4 powder looks clean. And small amounts of methylpropiophenone should not lead to such results.
 

w2x3f5

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Describe the synthesis technique you used.
Who is the supplier?
In appearance, BK4 powder looks clean. And small amounts of methylpropiophenone should not lead to such results.
HIGGS BOSSONI check with him. Standard 50 grams bk4+350 dcm+methylamine 40% 100 ml, 2 hours mixed, control temp 30 degrees.
In him 100 gr bk4 have around 15 ml methylpropiophenon, its not good. And washing in hot water not helped, maybe recristallyzation helps
 
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w2x3f5

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Why do you think it is 4-methylpropiophenone? @white7proton Have you measured melting point of BK4? In general, I agree with @HIGGS BOSSON . I guess you added too much acid. Have you measured pH while HCl 36% addition? Have you used HCl solution in acetone or added it without solvent. pH is very important and you could overoxydize your 4-MMC by fast addition of full volume HCl. Also, have you washed your 4-mmc free base by water from methylamine excess?
G.PattonYou upset me. The methylamine is washed out with high quality, the acid was used less than half of the theoretically required amount, the acid was added very slowly, with acetone it turns out blue shit (he already wrote with a photo in another post). If you take bk4 and melt it, it melts at approximately 56-60 degrees, but the author does not have the technical ability to melt the sample in a capillary as it should be done. But we all know perfectly well that the melt of bk4 in water should sink (for memory 1.4 g/ml), since its density is much higher than water (1 g/ml), and the density of the MP is 0.991 g/ml
 

G.Patton

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You upset me. The methylamine is washed out with high quality, the acid was used less than half of the theoretically required amount, the acid was added very slowly, with acetone it turns out blue shit (he already wrote with a photo in another post). If you take bk4 and melt it, it melts at approximately 56-60 degrees, but the author does not have the technical ability to melt the sample in a capillary as it should be done. But we all know perfectly well that the melt of bk4 in water should sink (for memory 1.4 g/ml), since its density is much higher than water (1 g/ml), and the density of the MP is 0.991 g/ml
w2x3f5
You upset me.
I guess I can overcome it
 

G.Patton

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You upset me. The methylamine is washed out with high quality, the acid was used less than half of the theoretically required amount, the acid was added very slowly, with acetone it turns out blue shit (he already wrote with a photo in another post). If you take bk4 and melt it, it melts at approximately 56-60 degrees, but the author does not have the technical ability to melt the sample in a capillary as it should be done. But we all know perfectly well that the melt of bk4 in water should sink (for memory 1.4 g/ml), since its density is much higher than water (1 g/ml), and the density of the MP is 0.991 g/ml
w2x3f54-methylpropiophenone has 238-239 7 °C melting point, BK4 has 75-77 °C melting point. You said that this product has 56-60 °C. Do you understand that it have to melt at higher temperature, not lower?
 
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w2x3f5

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4-methylpropiophenone has 238-239 °C melting point, BK4 has 75-77 °C melting point. You said that this product has 56-60 °C. Do you understand that it have to melt at higher temperature, not lower?
G.PattonY self checked BK4 has 75-77 °C ? 4-mp 238 its boiling point, you wrong
 

w2x3f5

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4-methylpropiophenone has 238-239 °C melting point, BK4 has 75-77 °C melting point. You said that this product has 56-60 °C. Do you understand that it have to melt at higher temperature, not lower?
G.PattonDo you understand that the unpurified product melts lower for everyone? Do you understand that bk4 manufacturers do not purify it and do not recrystallize it
 

G.Patton

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Do you understand that the unpurified product melts lower for everyone? Do you understand that bk4 manufacturers do not purify it and do not recrystallize it
w2x3f5
Do you understand that the unpurified product melts lower for everyone?
It is false. Product can be polluted by substances with higer mp. As you suppose in this case, it is 4-methylpropiophenone. Hence, mp of bk4 have to rise.
Do you understand that bk4 manufacturers do not purify it and do not recrystallize it
I don't know about this product any. As I understand, neither you. You have just assumptions. I would like to continue this discussion with topic author.
 
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w2x3f5

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It is false. Product can be polluted by substances with higer mp. As you suppose in this case, it is 4-methylpropiophenone. Hence, mp of bk4 have to rise.

I don't know about this product any. As I understand, neither you. You have just assumptions. I would like to continue this discussion with topic author.
G.PattonAnd the last moment, the author used water at 70 degrees (thermostat with a temperature sensor) and everything melted. Even according to your data, there is a problem with bk4
 

w2x3f5

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It is false. Product can be polluted by substances with higer mp. As you suppose in this case, it is 4-methylpropiophenone. Hence, mp of bk4 have to rise.

I don't know about this product any. As I understand, neither you. You have just assumptions. I would like to continue this discussion with topic author.
G.PattonMP is a liquid under normal conditions, you write that it melts at 238 degrees
 

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It is false. Product can be polluted by substances with higer mp. As you suppose in this case, it is 4-methylpropiophenone. Hence, mp of bk4 have to rise.

I don't know about this product any. As I understand, neither you. You have just assumptions. I would like to continue this discussion with topic author.
G.PattonBK4 will not rise, the density of its melt is more than 1 gram per milliliter))) your DCM does not rise to the top layer in pure water?)))
 

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MP is a liquid under normal conditions, you write that it melts at 238 degrees
w2x3f5Yes, you are right. My bad. Temperature have to down. Anyway, 4-BK may be recrystallized from benzene with slight warm.
 

w2x3f5

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Yes, you are right. My bad. Temperature have to down. Anyway, 4-BK may be recrystallized from benzene with slight warm.
G.Pattonno need benzene, for author its hazard, IPA best variant, I think work same great same like with p2np
 

white7proton

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Can someone help explain how I can clean the 2B4M so that it doesn't make my mix go black when I add acid.

I'm trying my best to liase with the seller, if you or someone can help with a method to fix / clean the 2B4M I have then I will be happy with that, I just want to fix it so I can finally finish my synthesis.

Or, you can do step by step with me, I will show photos and videos etc and do the whole process and show you that what I am saying is the truth. Please guys.
 

sierraleone

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Can someone help explain how I can clean the 2B4M so that it doesn't make my mix go black when I add acid.

I'm trying my best to liase with the seller, if you or someone can help with a method to fix / clean the 2B4M I have then I will be happy with that, I just want to fix it so I can finally finish my synthesis.

Or, you can do step by step with me, I will show photos and videos etc and do the whole process and show you that what I am saying is the truth. Please guys.
white7protonI'm sure the reason that you are getting black liquid is that you are adding acid too fast.
It must be added dropwise,very slowly while stirring vigorously.If you think you added it slowly do it even slower.
 
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G.Patton

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How better if he wash him layer 300 ml dcm with total 2 litters water? Its not MeNH2, just understand it pls
w2x3f5Okay, take it easy, man. You didn't mentioned about 2l water =/ I just want to help, ok?
 

w2x3f5

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Okay, take it easy, man. You didn't mentioned about 2l water =/ I just want to help, ok?
G.PattonProblem with BK4, please just check him photo and can see much mp because oil layer up (mp 0.991 gram/ml). Its seller problem
 

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pH Don't prove MeNH2 presence or absence. I recommend to wash it better and evaporate part of DCM with MeNH2 traces after washing by water.
G.Pattonprove if much MeNH2, if low yes y right
 

G.Patton

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Problem with BK4, please just check him photo and can see much mp because oil layer up (mp 0.991 gram/ml). Its seller problem
w2x3f5
mp 0.991 gram/ml
I asked about melting point, not about its density. Do you know about this chemical analysis method? It can help you to determine purity of substance indirectly. Also, I'm sure that problem not with BK4. Probably something wrong with acid or acetone.
prove if much MeNH2, if low yes y right
Sorry, I don't understand your statement
 

w2x3f5

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I asked about melting point, not about its density. Do you know about this chemical analysis method? It can help you to determine purity of substance indirectly. Also, I'm sure that problem not with BK4. Probably something wrong with acid or acetone.

Sorry, I don't understand your statement
G.PattonI think this question we closed, because problem with bk4. About chemistry we can talking in pm )
 

w2x3f5

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Another person has the same problem and contacted me. The seller is the same, the goods are the same and the problem is exactly the same. I hope the site administration will take action against the seller of low-quality goods to resolve the problem.
 

mocnykutas

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Made your self u get good
 

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w2x3f5

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Bro of course I do self, I not buy bk4, read good this topic )))
Its people buy from one seller in this board...
 
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